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To experimentally investigate evaporating sprays under conditions experienced in high speed direct-injection (HSDI) diesel engines, the exciplex LIF technique with the TMPD / naphthalene dopant system was applied in a combustion-type constant-volume spray chamber. The chamber allows spark ignition of a slightly rich C2H2-air mixture, and subsequent fuel injection into the high temperature and pressure products. A detailed set of calibration experiments has been performed in order to quantify the TMPD fluorescence signal. It has been demonstrated that the TMPD fluorescence intensity is directly proportional to concentration, is independent of the chamber pressure, and was not sensitive to quenching by either water vapor or carbon dioxide. Therefore, the temperature dependence of the TMPD fluorescence was the only correction factor required for quantitative measurements. Using a dual heated-jet experiment, the temperature dependence of TMPD fluorescence up to 1000 K was measured.